US3512569A - Detergent reactor - Google Patents

Description

CHUNG YU SHEN ETAL 3,512,569

May 19, 1970 DETERGENT REACTOR 3 Sheets-Sheet 1 Filed March 26, 1968 TUE INVENTOR CHUNG YU SHEN BY NORMAN E. STAHLHEBER ATTORNEY May 1970 CHUNG YU SHEN ETAL 3,512,569

DETERGENT REACTOR Filed March 26, 1968 3 Sheets-Sheet 2 FIG 3 "III II i

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DETERGENT REACTOR Filed March 26, 1968 s Sheets-Sheet 5 v INVENTOR CHUNG YU SHEN NORMAN H. STAHLHEBER MXM ATTORNEY United States Patent '0 3,512,569 DETERGENT REACTOR Chung Yu Shen, St. Louis, Mo., and Norman Earl Stablheber, Columbia, Ill., assignors to Monsanto Company, St. Louis, Mo., a corporation of Delaware Filed Mar. 26, 1968, Ser. No. 716,151 Int. Cl. B01d 1/14 US. Cl. 159--16 4 Claims ABSTRACT OF THE DISCLOSURE Apparatus useful in the production of solid detergent compositions comprising a reaction vessel having an expansion section and a mixing section and a means for injecting a gaseous drying medium at the internal lower portion of said reaction vessel. Preferred embodiments include additionally (a) a means for pivotally mounting said vessel, (b) a means for pivoting said vessel at least about 90 from an upright position and (c) an agitator that permits said pivoting located inside said mixing chamber.

This invention relates to an apparatus useful in the production of detergent compositions. More particularly, it relates to equipment useful in the production of detergent compositions from a process that utilizes an alkali metal trimetaphosphate as a raw material.

In detergent processes the use of trimetaphosphates wherein the trimetaphosphate ring is cleaved to form tripolyphosphates has many advantages over the use of tripolyphosphates. The detergent process generally utilizes several individual steps and requires separate pieces of equipment for each step. For example, the alkali metal trimetaphosphate is slurried with water and other conventional detergent ingredients in a mixer. Thereafter, the trimetaphosphate is reacted with a strong base in a separate reaction vessel and the material is generally foamed to a relatively light density product. Thereafter, the material is discharged and dried. While a continuous process is generally suitable for many detergent manufacturers, in some instances the change-over from one formulation to another is repetitive and causes a relatively large amount of downtime in order to clean the various pieces of equipment. There is a need for a single piece of apparatus in which all of the processing steps can be accomplished, that is, one vessel for the mixing, reacting and drying steps. It is believed, therefore, a single piece of equipment in which all of the steps can be carried out is an advancement in the art.

The present invention is a reaction vessel useful for the production of solid detergent materials comprising (a) a reaction vessel having a mixing section and an expansion section having a volumetric ratio of 1:1 to 1:4, respectively, and (b) injecting a gaseous drying medium at the lower internal portion of said reaction vessel. Preferred embodiments include the foregoing reactor equipped with (c) a means for pivotally mounting said vessel, (d) a mean for pivoting said vessel at least 90 from its upright position so that contents of the vessel are discharged from the open end and (e) an agitator located inside the vessel that permits the pivoting.

The reaction vessel will generally be round in shape; however, other geometric figures, such as ovals, hexagons, octagons and the like can be used with satisfactory results. It is preferred to use a shape having cylindrical sides with a conical, semi-spherical or dish type bottom since the contents will be more easily discharged from such a vessel at the completion of the cycle. Since the contents expand during the reaction from 2 to 5 times their original volume, the vessel is constructed to accommodate this expansion in volume. Because of this expansion in volume ice certain configurations have been found to be preferred embodiments. For example, one preferred configuration is to construct the vessel with a mixing chamber of a size suitable to accommodate the volume of ingredients then construct an expansion chamber having about 3 to 5 times the volume of the mixing chamber. Two embodiments of the foregoing construction of the expansion chamber have been found to be preferred. One embodiment is to have the expansion chamber above the mixing chamber which is cylindrical in shape. The diameter of the expansion chamber is at its largest diameter from 1.5 to about 2 times the diameter of the mixing chamber. The lower portion of the expansion chamber has a varying diameter and is used as a transition piece to connect to the mixing chamber. An additional preferred embodiment is to provide a concentric shell to encompass the mixing chamber. The annular spacing between the mixing chamber and the shell provides the expansion chamber which volume is from about 1.5 to about 5 times the volume of the mixing chamber. This embodiment enables good mixing design in the vessel independent of the additional volume required for expansion.

The vessel can be constructed from any metallic or glass-fiber-resin material which is desired, although generally carbon steel *will be preferred because of economics and in most instances, the reactants create no significant corrosion problems. The thickness of the vessel will bedependent upon the batch size desired. For example, 16 gauge steel is suitable for a vessel which will produce about 200 pounds of a typical detergent composition. One skilled in design can readily select the appropriate size by utilizing engineering principles from the detailed description contained herein.

A means for injecting a gaseous drying medium is provided at the lower internal portion of the reaction vessel. The gaseout drying mediums which can 'be used are in general those gases which are unreactive with the detergent and which will remove the moisture, that is those that are unsaturated with water vapor. In most instances, air, flue gas, carbon dioxide or nitrogen will be preferred. Of these, warm, relatively dry air will be especially preferred.

Various configurations of the drying medium injection means can be used. For example, an air sparger with a single outlet located at the lower portion of the vessel is suitable if the vessel is relatively small. Larger vessels generally require more than one sparger or a manifold which will yield a relatively uniform distribution of the drying medium throughout the lower section of the reaction vessel. A preferred embodiment is to equip the vessel with a mechanical agitation with a plurality of agitator blades which agitation shaft and blades have a passage for the drying medium. By this means a uniform distribution of the drying medium is achieved and the agitator can serve two functions, that is, provide agitation and the means for injecting the gaseous drying medium.

It is preferred to construct the reaction vessel having an open end which is the upper end of the vessel when the vessel is in an upright position and with a means for pivotally mounting said vessel located on the external surface of said vessel, a means for pivoting said vessel at least about from said upright position to thereby discharge the contents of said vessel from said open end, said means located on the external surface of said vessel and an agitator located inside said mixing chamber that permits said pivoting.

A pivotal mounting means is provided on one of the preferred embodiments and can be at any location on the vessel; however, for ease of pivoting, the mounting means is preferably along a horizontal axis which would pass through or relatively close to the center of gravity of the vessel at the time the contents of the vessel are to be 3 discharged. As can be appreciated the center of gravity of the vessel can change during the cycle depending upon the design of the vessel. For example, when the expansion chamber is above the mixing chamber at the time before the reaction has started, the center of gravity will be at a relatively low position, that is, in the mixing chamber but will shift upwards as the reaction proceeds and the contents expand. When the expansion chamber is the annular spacing outside the mixing chamber, the shift in center of gravity is not so pronounced. It is also to be noted that generally two bearings will provide the pivotal mounting means; however, a single mounting means in some instances can be used if desired. More than two bearing surfaces can be used; however, if more than two such mounting means are used, the means must permit the pivoting.

In the foregoing preferred embodiment a means for pivoting the vessel at least about 90 from its upright position is provided. Suitable means include a hand operated lever for relatively small vessels. For larger vessels a mechanical means for pivoting the vessel such as a gear train connected to a suitable power source is generally used. In general, the particular means used for pivoting the vessel will be dependent upon several factors such as the overall size of the vessel, location of the mounting means in reaction to the center of gravity and the degree of automation that is desired.

The preferred apparatus has an agitator located inside the vessel which agitator permits the vessel to be pivoted at least 90 from its upright position. Any conventional agitator can be used such as the anchor, impeller, or paddle types of agitators that will achieve a relatively uniform mixture prior to the chemical reaction. Normally it is desirable to equip the agitator with a type of coupling that enables the agitator shaft to be relatively easy and rapidly disconnected from the power source that is used to provide movement to the agitator. A guide or a second bearing is usually provided in order to enable a relatively rapid reconnection of the agitator shaft to the power source after the contents of the vessel have been discharged and the vessel is returned to its upright position. The type of bearings and couplings that are selected will be dependent upon several factors such as the overall size of the equipment, type of agitator selected, the detergent formulation desired and the like. As previously mentioned, a preferred agitator is one which also provides the means for injecting the drying medium into the lower portion of the reaction vessel.

The trimetaphosphate, water and the detergent ingredients are charged to the vessel. The temperature is raised to the reaction temperature, generally from about 50 C. to about 90 C. The strong base is then added and mixed with the trimetaphosphate and other ingredients. The agitator is then shut OH and in about 1 to 2 minutes the reaction of the strong base and trimetaphosphate causes the contents of the reactor to expand in volume and steam is evolved. The detergent material is then cooled and dried by injecting the drying medium through the material. After the drying, the material is cooled enough for the contents to be discharged. In the preferred embodiment the vessel is rotated at least 90 and its contents are discharged from the open end of the vessel. After the contents are emptied out of the vessel, it is returned to its upright position and another batch can be produced.

The invention will now be described with reference to the accompanying drawings in which:

FIG. 1 is a longitudinal sectional view of one embodiment of the apparatus of this invention wherein the expansion chamber is above the mixing chamber mounted in a conventional mounting frame.

FIG. 2 is a longitudinal sectional view of the same embodiment as shown in FIG. 1 only the reactor is rotated enabling contents of the reactor to be discharged.

FIG. 3 is a longitudinal sectional view of another embodiment wherein the expansion chamber surrounds the mixing chamber.

FIG. 4 is a longitudinal sectional view of the same embodiment as shown in FIG. 3 only the reactor is rotated enabling contents of the reactor to be discharged.

With particular reference to FIG. 1, the reaction vessel 1 is provided with an agitator 3 located inside the vessel to provide mixing in the mixing chamber 4. The agitator 3 is provided with a quick disconnect coupling 5 to enable pivoting. An expansion chamber 6 having a larger diameter and a transition portion 7 is located above the mixing chamber 4. The reactor is pivotally mounted on the mounting means 8. The means for rotating the vessel 9 is mounted on the side of the vessel to enable pivoting of the vessel to at least thereby discharging the contents from the open end 10 of the vessel 1 after the reaction and expansion has occurred. A sparger for injecting the drying medium 11 is provided for cooling and drying the product. The agitator shaft 13 is hollow and if desired, the drying medium supply 15 can be supplied to the shaft and the agitator blades 17 have openings to distribute the medium air relatively uniformly at the lower portion of the vessel 1.

With particular reference to FIG. 2, the vessel 1 is shown in a pivoted position. The agitator shaft 13 has been disconnected at the coupling 5. Force is applied to the means for pivoting the vessel 9 to move the vessel from its upright position. After the contents of the vessel are discharged through the open end of the vessel 10, a force is applied to the means for rotating the vessel 9 and the vessel 1 is rotated to the upright position.

With particular reference to FIG. 3, the reaction vessel 30 shown in an upright position is constructed with a mixing chamber 31 and an annular outer shell 32 concentrically positioned outside the mixing chamber 31 and pivotally mounted on dual support means 33' and 34. The annular spacing between the mixing chamber 31 and the outer shell 32 provides the expansion chamber 35. The agitator 36 and agitator shaft 37 can be moved vertically by a lifting means 38 enabling the vessel to rotate at least 90 to discharge the contents from the mixing chamber 31 and expansion chamber 35. The reactor can be rotated after the reaction is completed by turning the handle 39 which operates through a gear train to provide suflicient force for the rotation of the reactor. The agitator shaft 37 has an annular passageway to allow a drying medium such as air or flue gas to be distributed to the lower portion of the mixing chamber 31.

With particular reference to FIG. 4, the vessel 32 is shown in a pivoted position which enables contents of the vessel to be discharged. The agitator 36 is in a raised position and can be lowered after the contents are discharged by the motor 44 which rotates the pinion 45 causing the carriage 46 to move downward.

What is claimed is:

1. Apparatus useful in the production of a solid detergent composition comprising (a) a reaction vessel having an open end which is the upper end of said vessel when said vessel is in an upright position, said vessel having a mixing chamber and an expansion chamber; the ratio of the volume of said mixing chamber to said expansion chamber being from about 1:1 to 1:5, (b) means for pivotally mounting said reaction vessel located externally on said reaction vessel, (c) a means for pivoting said vessel at least 90 around an axis which is transverse to said vessel, (d) an agitator inside said vessel driven by power means above the vessel and equipped with a quick disconnect coupling that permits said pivoting and (e) the shaft for said agitator is hollow and said agitator provides said means for distributing a gaseous drying medium at the lower internal portion of said reactor.

2. An apparatus according to claim 1 wherein said reaction vessel comprises (a) a generally cylindrical mixing chamber, and (b) generally cylindrical expansion chamber above said mixing chamber when said vessel is in an upright position, said expansion chamber comprising an upper section having a larger diameter than said 5 mixing chamber and a transition section between said upper section and said mixing chamber; the ratio of the volume of said mixing chamber to said expansion chamber being from about 1:3 to 1:5.

3. An apparatus useful in the production of a solid detergent composition comprising (a) a reaction vessel having an open end which is the upper end of said vessel when said vessel is in an upright position, said vessel having a mixing chamber and an expansion chamber, (b)

means for injecting a gaseous drying medium at the lower 10 internal portion of said reactor, (c) means for pivotally mounting said reactor located externally on said reactor, ((1) a means for pivoting said vessel at least 90 around axis which is lateral to said vessel, (6) an agitator inside said vessel that permits said pivoting, (f) said mixing chamber is generally cylindrical and (g) a shell taller than said mixing chamber which is cylindrically positioned around said mixing chamber, to provide an annular space between said shell and said mixing chamber, the ratio of the volume of said mixing chamber to said annular space being from about 1:1 to about 1:5 to thereby provide expansion chamber.

4. An apparatus according to claim 3 wherein the shaft for said agitator is hollow and said agitator provides said means for injecting said drying medium.

References Cited UNITED STATES PATENTS 219,411 9/1879 Pond 15916 1,040,427 10/1912 Savage et a1. 159-34 X 1,136,277 4/1915 Schlueter 159-23 1,942,818 1/1934 Kern et al 15934 FOREIGN PATENTS 11,677 1846 Great Britain. 20,454 1901 Great Britain. 287,198 3/ 1928 Great Britain. 424,751 9/ 1947 Italy.

NORMAN YUDKOFF, Primary Examiner J. SOFER, Assistant Examiner U.S. Cl. X.R.

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